CN105738505B - The detection method of volatile flavor components in coriander - Google Patents
The detection method of volatile flavor components in coriander Download PDFInfo
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- CN105738505B CN105738505B CN201610076667.9A CN201610076667A CN105738505B CN 105738505 B CN105738505 B CN 105738505B CN 201610076667 A CN201610076667 A CN 201610076667A CN 105738505 B CN105738505 B CN 105738505B
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- 238000001514 detection method Methods 0.000 title claims abstract description 21
- 239000000796 flavoring agent Substances 0.000 title claims abstract description 21
- 235000019634 flavors Nutrition 0.000 title claims abstract description 21
- 229940029991 coriander extract Drugs 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000000605 extraction Methods 0.000 claims abstract description 21
- 235000015112 vegetable and seed oil Nutrition 0.000 claims abstract description 19
- 239000008158 vegetable oil Substances 0.000 claims abstract description 19
- 238000004451 qualitative analysis Methods 0.000 claims abstract description 11
- 238000001319 headspace solid-phase micro-extraction Methods 0.000 claims abstract description 10
- 238000004817 gas chromatography Methods 0.000 claims abstract description 6
- KSMVZQYAVGTKIV-UHFFFAOYSA-N decanal Chemical compound CCCCCCCCCC=O KSMVZQYAVGTKIV-UHFFFAOYSA-N 0.000 claims description 37
- 238000011084 recovery Methods 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 10
- 238000011088 calibration curve Methods 0.000 claims description 8
- 238000001819 mass spectrum Methods 0.000 claims description 8
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 7
- 238000004445 quantitative analysis Methods 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 4
- 238000002137 ultrasound extraction Methods 0.000 claims description 4
- 239000012159 carrier gas Substances 0.000 claims description 3
- 238000002474 experimental method Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
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- 238000012795 verification Methods 0.000 claims description 3
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- 239000008157 edible vegetable oil Substances 0.000 claims description 2
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- 238000005516 engineering process Methods 0.000 abstract description 7
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- 238000004949 mass spectrometry Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 26
- 150000002500 ions Chemical class 0.000 description 14
- 239000003205 fragrance Substances 0.000 description 6
- 238000004587 chromatography analysis Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 238000003859 hyphenated technique Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229920003266 Leaf® Polymers 0.000 description 2
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- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000003440 toxic substance Substances 0.000 description 2
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- 241000196324 Embryophyta Species 0.000 description 1
- 208000019331 Foodborne disease Diseases 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 201000005505 Measles Diseases 0.000 description 1
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- 206010037660 Pyrexia Diseases 0.000 description 1
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- 230000000202 analgesic effect Effects 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 235000013409 condiments Nutrition 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
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- 230000035619 diuresis Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 208000001848 dysentery Diseases 0.000 description 1
- 201000006549 dyspepsia Diseases 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
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- GYHFUZHODSMOHU-UHFFFAOYSA-N nonanal Chemical compound CCCCCCCCC=O GYHFUZHODSMOHU-UHFFFAOYSA-N 0.000 description 1
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- 210000002784 stomach Anatomy 0.000 description 1
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- 239000012085 test solution Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention discloses a kind of detection methods of volatile flavor components in coriander, the detection method includes sample extraction, qualitative analysis, quantitative determination, interpretation of result and result conversion, wherein sample extraction is to extract coriander using vegetable oil, and qualitative analysis is analyzed with gas chromatography combined with mass spectrometry technology using headspace solid-phase microextraction.The present invention detection method realize the enrichment method to low level of voltile ingredient in coriander extract, the operating time is short, and sample size is small, and high selectivity, separating capacity is strong, can efficient pollution-free extraction coriander in volatile ingredient.
Description
Technical field
The invention belongs to analytical chemistry and field of food detection, and in particular to the inspection of volatile flavor components in a kind of coriander
Survey method.
Background technology
Coriander contains abundant nutritional ingredient and health-care components, and Traditional Chinese Medicine is thought, coriander is warm-natured sweet in flavor, and energy stomach invigorating disappears
Food, sweating promoting eruption, diuresis defaecation, wind dispelling removing toxic substances etc. are mainly used for treating measles, indigestion, cold, popular sexuality
It emits, blood under fever and headache, dysentery, hypertension can also be treated, external application has analgesic effect, also has removing toxic substances to make certain food poisonings
With.Its coriander cauline leaf soft aroma and, be most common condiment and a kind of ideal food with healthcare function in people's diet
It is very popular with pungent perfume material, so developing a kind of coriander spicing oil and establishing the coriander volatilization of complete set
The detection method of property ingredient has good development prospect.
Invention content
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, provide that a kind of operating time is short, sample size
Small, high selectivity, separating capacity be strong, can volatility in the coriander of low level of voltile ingredient in the extraction coriander of efficient pollution-free
The detection method of fragrance component.
In order to solve the above technical problems, the present invention uses following technical scheme：
The detection method of volatile flavor components, includes the following steps in a kind of coriander：
(1) sample extraction：Coriander is extracted using vegetable oil, obtains coriander extract sample to be measured；
(2) qualitative analysis：Using headspace solid-phase microextraction and Gas chromatographyMass spectrometry to coriander extract to be measured
Sample carries out qualitative analysis；
(3) it quantitative determines：GC conditions identical with qualitative analysis in step (2) are kept, calibration curve method is passed through
Quantitative analysis is carried out to principal component capraldehyde in coriander extract sample to be measured；
(4) interpretation of result：Analysis method is quantitative determined by Precision Experiment, sample recovery rate experimental verification step (3)
Accuracy；
(5) result converts：According to calibration curve method, capraldehyde content is calculated, and calculates coriander recovery rate；
Standard curve A=bC+a；W=[(A-a) × V1×10-6]/(b×MAlways×W1)；
In formula, A is peak area, and a, b are related coefficient, and C is capraldehyde concentration μ g/mL, V in the sample1For vegetable oil volume
Number mL, W1For coriander extract total content area percent, M shared by capraldehydeAlwaysIt is coriander recovery rate for coriander quality g, W.
In above-mentioned coriander in the detection method of volatile flavor components, it is preferred that described to be measured in the step (2)
The extraction temperature of the headspace solid-phase microextraction of coriander extract sample is 50 DEG C~65 DEG C, and extraction time is 25min~35min,
Be enriched with coriander extract sample to be measured extraction needle gas chromatograph-mass spectrometer (GC-MS) injection port parsing the time be 3min~
5min。
In above-mentioned coriander in the detection method of volatile flavor components, it is preferred that the gas-chromatography-of the step (2)
In mass spectrometric hyphenated technique, the injector temperature of gas-chromatography is 230 DEG C~250 DEG C, using temperature programming, temperature programming it is initial
Temperature is 40 DEG C~60 DEG C, and the speed of temperature programming is 3 DEG C/min~7 DEG C/min, and temperature programming is to 240 DEG C~260 DEG C.
In above-mentioned coriander in the detection method of volatile flavor components, it is preferred that the gas-chromatography-of the step (2)
In mass spectrometric hyphenated technique, the carrier gas that gas-chromatography uses carries out color for helium, with the constant current mode of 1.0mL/min~2mL/min
Spectrum separation, split ratio 1: 1~5, sample size are 1 μ of μ L~10 L.
In above-mentioned coriander in the detection method of volatile flavor components, it is preferred that the gas-chromatography-of the step (2)
In mass spectrometric hyphenated technique, it is 70eV~100eV, ion that the ion source of mass spectrum unit, which uses EI ion source modules, ion source voltage,
Source temperature is 230 DEG C~260 DEG C.
In above-mentioned coriander in the detection method of volatile flavor components, it is preferred that in the step (1), the sample
Extraction includes following procedure：Coriander is mixed and smashed to pieces with vegetable oil, after ultrasonic extraction and press filtration, coriander to be measured is obtained and carries
Take object sample.
In above-mentioned coriander in the detection method of volatile flavor components, it is preferred that the quality of the coriander and vegetable oil
Volume ratio is 40g~60g: 60mL~90mL.
In above-mentioned coriander in the detection method of volatile flavor components, it is preferred that the technique item of the ultrasonic extraction
Part is：20 DEG C~50 DEG C of ultrasonic temperature, ultrasonic power 100W~400W, ultrasonic time 30min~100min.
The innovation of the present invention essentially consists in：
1, coriander fragrance component is directly extracted using vegetable oil；2, it is extracted in coriander using headspace solid-phase microextraction technology
Volatile ingredient；3, using calibration curve method, the quantitative analysis method of coriander volatile ingredient is detected with establishing complete set.
Compared with the prior art, the advantages of the present invention are as follows：
1, the present invention is using headspace solid-phase microextraction technology, the association of Gas chromatographyMass spectrometry and calibration curve method
Same-action qualitatively and quantitatively has detected the volatile flavor components in coriander.The present invention is carried using headspace solid-phase microextraction technology
The volatile ingredient in coriander is taken, the operating time is short, and sample size is small, no extractant, favorable reproducibility, high selectivity, collection sampling,
Extraction, enrichment method, sample introduction are in one, volatile ingredient that can be in the extraction coriander of efficient pollution-free.Using gas-chromatography-matter
Spectrum joint technology combines the efficient separating capacity of gas-chromatography and mass spectrography determines the ability of molecular structure, high sensitivity, and
It can confirm each chemical composition in coriander volatile ingredient in conjunction with related document by retrieving NIST02 spectrograms library.Using standard
Curve method detects the quantitative analysis method of coriander volatile ingredient with establishing complete set.
2, the present invention directly uses vegetable oil (preferably edible vegetable oil) to extract coriander fragrance component, can produce coriander fragrance
Flavored oils.Vegetable oil is used directly to extract coriander fragrance component, the chemical solvent of noresidue, more health-nutrition for extractant
Safety, and this method is simple and practicable, it is of low cost.
Description of the drawings
Fig. 1 is that the gas chromatography-mass spectrum of coriander extract sample volatile flavor components to be measured in the embodiment of the present invention 1 is total
Chromatography of ions figure.
Fig. 2 is vegetable oil blank total ion chromatogram.
Fig. 3 is that the gas chromatography-mass spectrum of coriander extract sample volatile flavor components to be measured in the embodiment of the present invention 2 is total
Chromatography of ions figure.
Specific implementation mode
Below in conjunction with Figure of description and specific preferred embodiment, the invention will be further described, but not therefore and
It limits the scope of the invention.
Material and instrument employed in following embodiment are commercially available.
Embodiment 1：
The detection method of volatile flavor components, includes the following steps in a kind of coriander of the present invention：
(1) sample extraction：The fresh coriander cauline leafs of 50g are cleaned, drain, are shredded, 75mL vegetable oil is added and smashs to pieces, then
Ultrasonic extraction, 35 DEG C, ultrasonic power 200W, ultrasonic time 50min of ultrasonic temperature, then press filtration are carried out, coriander extraction to be measured is obtained
Object sample.
(2) qualitative analysis：Qualitative analysis is carried out using headspace solid-phase microextraction and gas chromatograph-mass spectrometer (GC-MS).Take 5mL
Coriander extract sample to be measured is placed in ml headspace bottle, and 15min~30min, 50/30 μm of DVB- are preheated at 50 DEG C~65 DEG C
CAR-PDMS extraction needles extract 30min at 60 DEG C, and the injection port parsing time of gas chromatograph-mass spectrometer (GC-MS) is 3min.Gas
The injector temperature of phase chromatography is 250 DEG C, and using temperature programming, initial temperature is 60 DEG C, and temperature programming speed is 5 DEG C/min,
To 260 DEG C, helium is carrier gas for temperature programming, and chromatographic isolation, split ratio 1: 1, sample introduction are carried out with the constant current mode of 1.0mL/min
Amount is 1 μ L.It is 230 DEG C that the ion source of mass spectrum unit, which uses EI ion source modules, ion source voltage 70eV, ion source temperature,.
As shown in Figure 1, for the gas chromatography-mass spectrum total ion chromatogram of coriander extract volatile flavor components in the present embodiment, Fig. 2
For vegetable oil blank total ion chromatogram.(unknown be blank to each volatile compound component list in the present embodiment coriander extract
Sample) as shown in table 1.
Each volatile compound component list in 1 embodiment of table, 1 coriander extract (unknown is blank sample)
(3) it quantitative determines：GC conditions identical with qualitative analysis are kept, calibration curve method FID (hydrogen fire is passed through
Flame ionisation detector) quantitative analysis is carried out to coriander extract principal component capraldehyde standard specimen.Using capraldehyde mass concentration as abscissa,
Corresponding peak area is that ordinate carries out linear regression, equation of linear regression A=121875.3022C+5000000.
(4) interpretation of result：The accuracy of analysis method, tool are quantitative determined by precision, sample recovery rate experimental verification
Gymnastics is made as follows：
(4.1) Precision Experiment：The personnel respectively parallel capraldehyde plant for preparing the 0.664mg/mL containing capraldehyde is analyzed by two
Each 6 parts of oily mixed solution.The precision test solution respectively prepared is measured on two different chromatographs.Two people respectively survey
The relative standard deviation for obtaining 6 parts of solution recoveries is respectively 2.8% and 4.2%, is shown good using the repeatability of this method；Two
The relative standard deviation of 12 parts of capraldehyde vegetable oil mixed solution rate of recovery data measured by the analysis personnel of position is 3.8%, is shown
It is good using the Intermediate precision of this method.
(4.2) sample recovery rate is tested：Different amounts of capraldehyde vegetable oil mixed solution is separately added into sample, preparation contains
Capraldehyde is the solution of basic, normal, high 3 kinds of concentration, and three parts are averagely prepared under each concentration, and measuring capraldehyde by area normalization method contains
Amount, calculates the rate of recovery of capraldehyde, the results are shown in Table 2.
2 sample recovery rate experimental result table of table
(5) result converts：According to calibration curve method, unknown extract capraldehyde and aldehyde C-9 content are calculated, and calculate excess of export
Sound extracts the recovery rate of coriander.
Standard curve A=bC+a；W=[(A-a) × V1×10-6]/(b×MAlways×W1)。
In formula, A is peak area, and a, b are related coefficient, and C is the concentration (μ g/mL) of capraldehyde in the sample, V1For vegetable oil
Volume number (mL), W1For coriander extract total content area percent, M shared by capraldehydeAlwaysFor coriander quality (g), W extracts for coriander
Rate.
By calculating, the recovery rate of coriander is 0.0862% in the present embodiment.
Embodiment 2：
The detection method of volatile flavor components in a kind of coriander of the present invention, with essentially identical, area the step of embodiment 1
It is not only that：Coriander quality is 40g.
Fig. 3 is coriander extract volatile ingredient gas chromatography-mass spectrum total ion chromatogram in the embodiment of the present invention 2.
By calculating, the recovery rate of coriander is 0.0736% in the present embodiment.
The present invention proposes a kind of extraction preparation method of new coriander fragrance, and by the detection to volatile ingredient,
Using headspace solid-phase microextraction technology and Gas chromatographyMass spectrometry to head space equilibrium temperature and time and chromatographic condition
Grope, it is determined that optimal gas chromatography-mass spectrum separation condition, it is determined that detect to complete set determining for coriander volatile ingredient
Property quantitative analysis method.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example.All technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It is noted that for the art
Those of ordinary skill for, improvements and modifications without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (2)
1. the detection method of volatile flavor components, includes the following steps in a kind of coriander：
（1）Sample extraction：Coriander is extracted using vegetable oil, the vegetable oil is edible vegetable oil, obtains coriander to be measured
Extract sample；
（2）Qualitative analysis：Using headspace solid-phase microextraction and Gas chromatographyMass spectrometry to coriander extract sample to be measured
Carry out qualitative analysis；
（3）Quantitative determination：Holding and step（2）The identical GC conditions of middle qualitative analysis, are treated by calibration curve method
It surveys principal component capraldehyde in coriander extract sample and carries out quantitative analysis；
（4）Interpretation of result：Pass through Precision Experiment, sample recovery rate experimental verification step（3）Quantitative determine the standard of analysis method
True property；
（5）As a result it converts：According to calibration curve method, capraldehyde content is calculated, and calculates coriander recovery rate；
Standard curve A=bC+a；W=[(A-a)×V1×10-6]/（b×MAlways×W1）；
In formula, A is peak area, and a, b are related coefficient, and C is capraldehyde concentration μ g/mL, V in the sample1For vegetable oils product mL,
W1For coriander extract total content area percent, M shared by capraldehydeAlwaysIt is coriander recovery rate for coriander quality g, W；
The step（2）In, the extraction temperature of the headspace solid-phase microextraction of the coriander extract sample to be measured is 50 DEG C~65
DEG C, extraction time is 25min~35min, is enriched with the extraction needle of coriander extract sample to be measured in gas chromatography-mass spectrography
The injection port parsing time of instrument is 3min~5min；
The step（2）Gas chromatographyMass spectrometry in, the injector temperature of gas-chromatography is 230 DEG C~250 DEG C,
Using temperature programming, the initial temperature of temperature programming is 40 DEG C~60 DEG C, and the speed of temperature programming is 3 DEG C/min~7 DEG C/min,
Temperature programming is to 240 DEG C~260 DEG C；
The step（2）Gas chromatographyMass spectrometry in, the ion source of mass spectrum unit uses EI ion source modules, from
Component voltage is 70eV~100eV, and ion source temperature is 230 DEG C~260 DEG C；
The step（1）In, the sample extraction includes following procedure：Coriander is mixed and smashed to pieces with vegetable oil, through ultrasonic wave
After extraction and press filtration, coriander extract sample to be measured is obtained；
The mass volume ratio of the coriander and vegetable oil is 40g~60g: 60mL~90mL；
The process conditions of the ultrasonic extraction are：20 DEG C~50 DEG C, ultrasonic power 100W~400W of ultrasonic temperature, ultrasonic time
30min~100min.
2. the detection method of volatile flavor components in coriander according to claim 1, which is characterized in that the step
（2）Gas chromatographyMass spectrometry in, the carrier gas that gas-chromatography uses is helium, with 1.0mL/min~2mL/min's
Constant current mode carries out chromatographic isolation, split ratio 1: 1~5, and sample size is 1 μ of μ L~10 L.
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